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1、Co含量对玻璃光度指标的影响摘 要熔制玻璃时加入少量玻璃着色剂，可制得各种有色玻璃。玻璃的着色不仅关系到各种颜色玻璃的生产，也是一种研究玻璃结构的手段。对着色玻璃，大家更关注玻璃的色度指标，但对玻璃的光度指标的影响因素相关研究不多。本文通过改变钴玻璃中钴含量、氧化还原剂用量、K2O用量来熔制玻璃样片，同时检验玻璃的热历史，然后用SP1920型分光光度计对玻璃样片进行光谱曲线的绘制分析。结果表明：着色剂用量、K2O的添加量及玻璃的热历史均对玻璃光谱曲线有较大影响,配合料的氧化还原气氛对该玻璃的光谱曲线影响不大。关键词：钴玻璃，熔制，光度指标，光谱曲线 Cobalt content on the
2、influence of glass photometric indexABSTRACTWhen a small amount of melting glass, glass coloring agents, can be obtained by a variety of colored glass. Colored glass of various colors of glass not only to the production, but also a means of discussing glass structure. Of colored glass, we are more c
3、oncerned about the color index of glass, but the luminosity of glass studies factors Index few. By changing the cobalt glass cobalt oxide reducing agent, K2O content to melt glass samples, also examined the thermal history of glass, and then use SP-1920 spectrophotometer spectral curves of glass sam
4、ples for analysis. The results showed that: the amount of coloring agent, K2O of addition and thermal history of glass were on the spectral curve of the glass have a greater impact, with the atmosphere of the redox material spectral curve of the glass has little effect. KEY WORDS: cobalt glass，melti
5、ng，brightness index，spectral curve8目录前言1第1章 实验21.1 实验原料及所用设备21.1.1实验原料21.1.2所用设备21.2玻璃的熔制21.2.1 CoO用量实验21.2.2 玻璃配合料氧化还原气氛熔制实验31.2.3 热历史实验31.2.4 K2O用量实验3第2章 结果与讨论52.1钴含量引起光度指标的变化52.2 氧化还原气氛对玻璃光谱曲线的影响52.3玻璃的热历史对玻璃光谱曲线的影响62.4碱金属（K2O）含量不同对玻璃光谱曲线的影响7结论9谢 辞10参考文献11附录13外文资料翻译15前言玻璃对可见光的透过率是其主要的价值性能。颜色玻璃或带有
6、某种“色调”的玻璃则多少不等而有选择性地影响透过率。玻璃着色后一般仍然保持透明，可是有些元素（Mn,Co）的着色能力很强，含有这些元素的玻璃，虽然浓度很低，厚度也很普通，已可能不透明。因此为了在生产过程中控制好色度指标的同时也更好的控制光度指标，该项目将系统的研究着色玻璃透光率的影响因素。希望能够提供一些光度指标的变化规律，减少生产的盲目性。本文通过改变着色剂含量、氧化还原剂用量、K2O用量以及热历史来熔制有色玻璃样片并用分光光度计对玻璃样片进行光谱曲线的绘制。然后对测得的光谱曲线进行分析，总结出这些因素对钴玻璃光度指标的影响规律，用于指导生产。 第1章 实验1.1 实验原料及所用设备1.1.
7、1实验原料矿石原料包括硅砂、白云石、石灰石、长石、萤石五种；化工原料包括碳酸钠（Na2CO3）、硫酸钠（Na2SO4）、硝酸钠（NaNO3）、氧化钴（CoO）、氧化钾（K2O）1。1.1.2所用设备 WAS50005电子天平，SGM3816C箱式电阻炉，SP-1920分光光度计，脱脂棉，镊子，酒精。1.2玻璃的熔制按玻璃的基础配方对各种原料进行准确称量后配制成配合料、再与着色剂混匀，将混匀后的配合料转入刚玉坩埚中，在高温炉中熔制2h，熔化温度为1450-1480，分别将样品1,2,3,4,5,6,7,8的熔融液倒入保温600的长方形模具中，样品6梯度降温至室温，其余样品保温1h后自然冷却至室温
8、。然后从模具中取出1001005玻璃制品，试样进行研磨抛光后，在SP-1920分光光度计上进行透光度的测定及光谱曲线的绘制2。1.2.1 CoO用量实验3保持其他成分不变，着色剂（CoO）用量见下表1-1，按1.2中步骤熔制，对应得到的玻璃编号为1、2、3。用SP-1920分光光度计对玻璃样片进行光度指标的测定。表1-1 着色剂用量Sample CoO（%）COD备注10.003228.9020.006228.9030.009228.901.2.2 玻璃配合料氧化还原气氛熔制实验实验中氧化性控制剂用量见下表1-2，其他基本成分条件相同，按1.2中步骤熔制，熔制后对应得到4、5样片。表1-2氧化
9、剂用量SampleCoO（%）NaNO3备注4 0.0060.250.0060.41.2.3 热历史实验保持其他成分和条件不变，按1.2中步骤熔制，冷却过程采用阶梯降温，温度由1455冷却至1200，冷却时间为1h，采用梯度降温至800，最后冷却至室温，对应得到6样片，其中氧化钴含量如下表1-3。表1-3热历史 SampleCoO（%）COD备注60.006228.90检验热历史1.2.4 K2O用量实验保持其他成分和条件不变，加入等量氧化钴，碱金属（K2O）用量见表1-4，按1.2中步骤熔制，对应得到7、8样片。表1-4 K2O用量SampleCoO（%）COD备注70.006228.90加
10、入1% K2O80.006228.90加入3%K2O 第2章 结果与讨论2.1钴含量引起光度指标的变化对1、2、3样片分别进行光谱曲线的测定，结果如下图21所示。由下图可见，随着着色剂（CoO）用量的增加，可见光区的透光率下降。原因可能是：玻璃的着色是由于可见光透过玻璃时，不同波长透过程度不同而产生的，究其原因是由于溶解在玻璃中的过渡金属离子（Co2+）的电子跃迁而引起的光吸收，着色离子（Co2+）浓度高，钴玻璃的光吸收越强，则透过率就越低。透光度与着色离子浓度的关系可用下式表示4。T=e-kcd d式样厚度；k分子消光度；c离子浓度图2-1 不同着色剂（CoO）含量的玻璃透光率与波长的关系2
11、.2 氧化还原气氛对玻璃光谱曲线的影响保持基础成分和着色剂用量相同，2样片熔制过程不加氧化剂（NaNO3），4样片加入0.2氧化剂（NaNO3），5样片加入0.4氧化剂（NaNO3）。用SP-1920分光光度计分别对2,4,5样片进行光谱曲线的测定，结果如下图2-2，由图可知样片2,4,5在波长607 nm处的透光度分别为38，38，44，随着氧化剂（NaNO3）用量的增加，样片的透光率变化不大。由此判断氧化钴是比较稳定的强着色剂，光谱曲线受氧化还原气氛的影响不大5。图2-2 不同氧化剂（硝酸钠）用量时玻璃透光率与波长的关系2.3玻璃的热历史对玻璃光谱曲线的影响熔制6样片过程采用阶梯降温，熔制
12、2样片时仍旧采用正常降温。用SP-1920分光光度计分别对2,6样片进行光谱曲线的测定结果如图23所示。由图可知，在同一波长处，采用阶梯降温的钴玻璃样片6的透光率低于正常降温的玻璃样片2。在退火温度范围内，保持一定温度，其趋向平衡折射率的速率与所处的温度有关。当玻璃在退火温度范围内，保持一定温度与时间并达到平衡折射率后，不同的冷却速度得到不同的折射率。冷却速度愈快，折射率愈低；冷却速度愈慢，折射率愈高。由于Co2+在玻璃中以CoO6和 CoO4两种状态存在，高温有利于低配位的CoO4低温有利于高配位的CoO6。综上所述玻璃的热历史对玻璃光谱曲线有一定的影响。图2-3 不同冷却方法时玻璃透光率与
13、波长的关系2.4碱金属（K2O）含量不同对玻璃光谱曲线的影响2样片配合料中不加碱金属（K2O），7样片配合料中加1%K2O ，8样片配合料中加3%K2O，用SP-1920分光光度计对上述样片进行透光率的测定及光谱曲线的绘制结果如下图，由图可知：在一定波长范围内，在同一波长处，随着碱金属（K2O）含量的升高，钴玻璃的透光率升高。究其原因是：玻璃中的钴一般以CoO6和CoO4两种形式存在，随着K2O的增加会促使CoO6向CoO4转变，从而导致降低CoO6的含量，随着CoO6的减少其电子发生跃迁时所吸收的能量也随着降低, 即对通过玻璃的可见光吸收也就随之降低，从而导致玻璃的透光率增加。同时K2O能防
14、止不混溶相导致的析晶,进而防止产生浑浊。 图2-4 不同碱金属（K2O）含量时玻璃透光率与波长的关系结论由以上实验可以得出如下结论:着色剂（CoO）用量对该玻璃的光度指标影响较大，在一定范围内，随着着色离子浓度的增加，透光率在下降;熔制过程中氧化还原气氛对该玻璃的光谱曲线影响不大；玻璃的热历史对该玻璃有一定的影响；碱金属（K2O）含量对该玻璃的光谱曲线有一定的影响，在一定范围内，随着碱金属（K2O）含量的升高，该玻璃的透光率升高。该研究方法还存在一定的不足之处，测得的光谱曲线可能由于某些原因存在一定的误差。影响钴玻璃的光谱曲线的因素还有很多，我们仍旧需要进一步的研究。9谢 辞非常感谢白老师指引
15、我们的论文的写作的方向和架构，并对本论文初稿进行认真批阅，指正出其中误谬之处，使我们有了思考的方向。谨向白老师表示崇高的敬意和衷心的感谢！谢谢白老师在我们撰写论文的过程中给与我的极大地帮助。 还有，要感谢在大学期间所有传授我们知识的老师，是你们的悉心教导使我们有了良好的专业课知识，这也是论文得以完成的基础。 感谢所有给我们帮助的老师和同学，谢谢你们！ 通过此次的论文，我们学到了很多知识，跨越了传统方式下的教与学的体制束缚，在论文的写作过程中，通过查资料和搜集有关的文献，培养了自学能力和动手能力。并且由原先的被动的接受知识转换为主动的寻求知识，这可以说是学习方法上的一个很大的突破。在以往的传统的
16、学习模式下，我们可能会记住很多的书本知识，但是通过毕业论文，我们学会了如何将学到的知识转化为自己的东西，学会了怎么更好的处理知识和实践相结合的问题。 在论文的写作过程中也学到了做任何事情所要有的态度和心态，首先做学问要一丝不苟，对于发展过程中出现的任何问题和偏差都不要轻视，要通过正确的途径去解决，在做事情的过程中要有耐心和毅力，不要一遇到困难就打退堂鼓，只要坚持下去就可以找到解决问题的思路。而且要学会与人合作，这样做起事情来就可以事倍功半。 总之，此次论文的写作过程，我们收获了很多，即为大学三年划上了一个完美的句号，也为将来的人生之路做好了一个很好的铺垫。 再次感谢我的大学和所有帮助过我并给我
17、鼓励的老师，同学和朋友，谢谢你们！ 30参考文献1 江宏, 王桂荣, ，韩新生等.浮法玻璃原料.北京：化学工业出版社，2006, 3-5.2 陈国平.玻璃的配料与熔制.北京：化学工业出版社，68-135. 3 陈福, 武丽华，赵思录.颜色玻璃概论.北京：化学工业出版社，2008,93-954 作花济夫，境野照雄，高桥克明（日本）.玻璃手册.中国建筑工业出版社, 1977，489-491.5 代春梅，李金平.无碱玻璃配合料熔化过程中的物化反应和能量消耗叶腊石与高岭土和石英砂组合之间的比较.硅酸盐学报，2011,39(4):652-656.6 曹文聪，杨树森.普通硅酸盐工艺学. 武汉：武汉理工大学
18、出版社,2009,139-151.7 赵彦钊，殷海荣主编.玻璃工艺学.北京:化学工业出版社，2006,12-13.8 陈福, 武丽华，赵思录.颜色玻璃概论.北京：化学工业出版社，2008,93-959 作花济夫，境野照雄，高桥克明（日本）.玻璃手册.中国建筑工业出版社, 1977，489-491.10 刘新年，赵彦钊.玻璃工艺综合实验.北京：化学工业出版社，2005,57-60.11 干福熹.玻璃的光学和光谱性质.上海：上海科学技术出版社,1991,201-219.12 朱仁萍，徐光青，吴玉程，廖延亮，王阳山，郑治祥.硼砂对粉煤灰多孔玻璃结构及性能的影响.硅酸盐通报，2011,30(1):17
19、7-181.13 金怀东，向卫东，黄海宇，杨帆，华伟，梁晓娟，董永军.Ce:YAG微晶玻璃制备及光谱性能.硅酸盐学报，2011,39(4):646-651.14 代春梅，李金平.无碱玻璃配合料熔化过程中的物化反应和能量消耗叶腊石与高岭土和石英砂组合之间的比较.硅酸盐学报，2011,39(4):652-656.15 藤宇，周佳佳，林耿，姜雄伟，邱建荣.玻璃激光内雕技术的最新进展. 硅酸盐学报，2011,39(4):657-661.16 朱军，戴世勋，吴礼刚，张魏，沈祥，王训国，徐铁锋，聂秋华.HO3+，Tm3+共掺GeGaSCsI玻璃的200m中红外发光特性的研究.光谱学与光谱分析.2011,3
20、1(4):894-897.17 祝君烨.微晶玻璃形成与着色研究硕士学位论文.清华大学，北京，1996.18 李志进，陈奇.铒对钠钙硅玻璃光谱性能的影响.玻璃与搪瓷，2010,38(4):17-21.19 孙成果，宁伟，汪庆卫.锑红宝石玻璃的研制与讨论.玻璃与搪瓷，2007,35(2):10-14.20 GB/T187012002.中华人民共和国国家标准.附录 中华人民共和国国家标准 着色玻璃 GB/T1870120021 范围 本标准规定了着色玻璃的分类、要求、检验规划、标志、包装、运输和贮存。 本标准适用于基体着色的浮法玻璃和普通平板玻璃。2 引用标准下列标准所包含的条文,通过在本标准中引用
21、而构成为本标准的条文本。标准出版时，所示版本均为有效。所有标准都会被修订,使用本标准的各方应探讨使用下列标准最新版本的可能性。GB/T26801994 建筑玻璃可见光透射比、太阳光直接透射比、太阳能总透射比、紫外线透射比及有关窗玻璃参数的测定（neq ISO 9095:1990）GB48711995 普通平板玻璃GB116141999 浮法玻璃GB/T119421989 彩色建筑材料色度测量方法3 分类 3.1着色玻璃按生产工艺分为着色浮法玻璃和着色普通平板玻璃。 3.2着色浮法玻璃按用途分为制镜级、汽车级、建筑级。着色平板玻璃按GB4871划分等级。 3.3着色玻璃按色调分为不同的颜色系列，
22、包括茶色系列、金色系列、绿色系列、蓝色系列、紫色系列、灰色系列、红色系列等。 3.4着色浮法玻璃按厚度分为以下种类：2mm,3mm,4mm，5mm,6mm,8mm,10mm,12mm,15mm,19mm。 着色普通平板玻璃厚度分2mm,3mm，4mm,5mm4 要求 4.1尺寸允许偏差、厚度允许偏差、对角线差、弯曲度。 着色浮法玻璃应符合GB11614相应级别的规定。着色普通平板玻璃应符合GB4871相应级别的规定。 4.2 外观质量 着色普通平板玻璃外观质量应符合GB4871相应级别的规定。 着色浮法玻璃外观质量中，光学变形的入射角各级别均降低5度，其余各项指标均应符合GB11614相应级别
23、的规定。4.3 光学性能 2mm,3mm,4mm,5mm,6mm着色浮法玻璃及着色普通平板玻璃的可见光透射比均不低于25%; 8mm,10mm,12mm,15mm,19mm的着色浮法玻璃的可见光透射比均不低于18%。中华人民共和国国家质量监督检验检疫总局2002-04-09批准 2002-10-01实施 外文资料翻译 Vol.24 No.2 SHEN Zuwu et al: Effect of Additional Applied ThermalDOI 10.1007/s11595-009-2308-9Effect of Additional Applied Thermal/Electric
24、Field onthe Float-glass SurfaceSHEN Zuwu1, LIU Qiming2*, MENG Li2, WANG Hongcheng 1,2(1. School of Mechanical and Electronic Engineering, Wuhan University of Technology, Wuhan 430070, China;2. Key Laboratory of Silicate Materials Science and Engineering (Wuhan University of Technology), Ministry of
25、Education, Wuhan 430070, China)Abstracts: The chemical resistances of float-glasses subjected to different electric field strength and temperature were investigated. It is indicated that the chemical resistance increases after the float-glasses are annealed with suitable temperature and electric fie
26、ld strength. It is also observed that the Na+ content varies obviously under the conditions of 570 , 1500 V/cm and 10 min, implying that the application of thermal/electric field improves the chemical resistance of float-glass online.Key words: float-glass; chemical resistance; thermal/electric fiel
27、d 1 IntroductionThe float glass process, developed several decades ago by Pilkington Brothers, Ltd., allows for the production of flat glass with an excellent surface finish which is processed continuously without no extra processing steps. The float process involves floating a ribbon of molten glas
28、s on a bath of molten tin1-3. The weathering and deterioration of alkali silicate glasses by humidity is a common problem now, especially for freshly formed surfaces (eg, blown bottles, fiberglass insulation wool and float-glass) under the hot and humid conditions of summer climate and warehouse sto
29、rage. The consequences of weathering can be nonuniform dimming or iridescence as well as staining or pitting, ie, visual defects and loss of strength. Prevopis investigations showed that the weathering of common soda-lime-silica glass was dominated by an ion exchange mechanism, where the network mod
30、ifiers Na+ as well as Ca2+ were leached out of the glass and hydrogen or hydrogen bearing species were incorporated into the silicate structure4-14. The weathering and corrosion mechanisms, especially in the case of soda-lime-silica float glass, were studied15. The physical and chemical adsorptions
31、of water are the first steps in the weathering process. The presence of unsatisfied network bonds and the coordinated sodium and calcium ions in the surface provides the primary driving force for physical adsorption of water. And then the subsequent chemisorption of water to form surface silanols is
32、 facilitated by nonbridging oxygens on the surface and in the bulk of the glass.The first description of water attacking on glass was developed by Doremus16, who considered the phenomenon as an exchange mechanism between water protons and alkali ions (sodium or potassium): 2H2O H3O+ + OH SiOR+ +H3O+
33、 +OH SiOH3O+R+ +OH Smets and Lommen developed the second model【27】as follows: SiOR+ + H2O SiOH + R+ + OHAccording to the second mechanism, the water molecule enters the network without previous dissociation.The global effect is the same in both models: there is a global increase in surface pH that i
34、nduces weathering. General surface ion loss by washing away induces further migration of alkaline and alkaline earth ions from bulk to surface, which increases the deeper corrosion of the glass.Generally, the weathering model is extremely complex under natural conditions due to the various parameter
35、s influencing the system. The thickness and the corrosion of the water film adsorbed on the glass surfaces eg, depends not only on the (micro)climate (relative humidity, temperature, atmospheric pressure, etc) but also on the content of acidic gases in the ambient atmosphere.The aim of this work was
36、 to demonstrate whether a suitable thermal/electric field reduces the content of sodium ion, which will reduce effectually the weathering of float-glass.2 ExperimentalCommercial 10 mm 10 mm 4 mm soda-limesilica float glass (nominal composition 71.50wt% -72.50wt% SiO2, 13.50wt%-14.00wt% Na2O, 8.00%-9
37、.00wt% CaO, 3.50wt%-4.00wt% MgO and a small amount of other elements, eg, Al2O3, Fe2O3, SO3) was used study. The tin side of the glass was made sign when it was cutting from the float glass production line. Subsequent fracture tests were performed on the glass plates before treated in the electrical
38、 field (untreated specimens) and after treated in the electrical field (treated specimens).Fig.1 schematically illustrates the applied thermal/ electrical field to induce alkali ions transferring from the surface to inside of glass. As a result of the process, the surfaces of the float glass are che
39、mically different. Because the surface (tin side) contains a significantamount of tin diffused into the surface (15-20 m), there are some adsorbed tinions on the other surface (air side), but it is negligible compared with the tin side. The presence of tin in the tin side leads to better weathering
40、resistance compared with the air side, so the air side was placed face to the positive electrode.The temperature varied from 450 to 570 in four steps (450 , 500 , 550 , and 570 ) and the electric field also varied from 1500 to 2400 V/cm in four steps (1500 V/cm, 1800 V/cm, 2100 V/cm, and 2400 V/cm).
41、 The 5 mm stainless steel were used as the electrodes. The glass samples were firstly treated by anhydrous alcohol, and then were treated by a one-stage heat-treatment (Fig.2). During the soaking time, a dc electric field was applied. The magnitude of the applied electrical field ranged from 1500 to
42、 2400 V/cm. The treated glass samples were also treated again by anhydrous alcohol and dried in the oven, and then bundled every two same treated glass samples up with adhesive tape and wire. It was similar to the situation in the warehouse storage. Intensified weathering was actualized in a machine
43、 with constant temperature and constant humidistat. Testing temperature was 85 , testing relative humidity was 95%, and testing time was 10 days.The treated glass samples were also treated again by anhydrous alcohol and dried in the oven, and then bundled every two same treated glass samples up with
44、 adhesive tape and wire. It was similar to the situation in the warehouse storage. Intensified weathering was actualized in a machine with constant temperature and constant humidistat. Testing temperature was 85 , testing relative humidity was 95%, and testing time was 10 days.The change of Na+ tran
45、sferred from surface to bulk was estimated by analyzing the change of SiOR+ peak and SiOSi peak using an infrared reflection spectrometer (IRRS) (VERTEX 70, Bruker, Germany). It was also estimated by analyzing the reflectance and transmittance using an NKD-system spectrophotometer (nkd-7000, Aquila,
46、 UK). While glow discharge-optical emission spectrometry (GD-OES) (Gdprofiller, Jobin Yvon, French)analysis was used as verifying method to study the variation of element contents on the quality of float-glass surface layers (several micros).A forward metallographic microscope (XJZ-6, Nanjing, China
47、) was also employed to explore the situationof weathered glass samples surface.3 Results and Discussionand the surface structure become loosen in the annealing furnace18. So the reflec Fig.3 shows the IRRS spectra of the glass samples treated at 450-570 for 10 min, respectively. It is observed that there a